Near infrared reflectance (NIR) spectroscopy was used to determine paracetamol, caffeine and lactose based excipient content of powders for direct compression and in intact tablet formulations as well. The nominal concentrations of the active moiety was different in each sample set, and calibration was carried out by multiple linear regression calculations from the reflectance spectral data. The results obtained with NIR spectroscopy were comparable with those obtained with high-performance liquid chromatography (HPLC) used as reference method. The non-destructive NIR method applied is thus suitable for the alternative quantitative determination of paracetamol, caffeine and additionally the excipient in intact tablets and have the advantage over HPLC of being rapid and can be simply carried out without sample preparation and without the use of any reagent.